EP0340279B1 - Uv scanning system for centrifuge - Google Patents

Uv scanning system for centrifuge Download PDF

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Publication number
EP0340279B1
EP0340279B1 EP88909862A EP88909862A EP0340279B1 EP 0340279 B1 EP0340279 B1 EP 0340279B1 EP 88909862 A EP88909862 A EP 88909862A EP 88909862 A EP88909862 A EP 88909862A EP 0340279 B1 EP0340279 B1 EP 0340279B1
Authority
EP
European Patent Office
Prior art keywords
sample
light
mirror
curvature
rotor
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
EP88909862A
Other languages
German (de)
English (en)
French (fr)
Other versions
EP0340279A1 (en
Inventor
Robert Giebeler
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Beckman Coulter Inc
Original Assignee
Beckman Instruments Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Beckman Instruments Inc filed Critical Beckman Instruments Inc
Publication of EP0340279A1 publication Critical patent/EP0340279A1/en
Application granted granted Critical
Publication of EP0340279B1 publication Critical patent/EP0340279B1/en
Expired legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/04—Investigating sedimentation of particle suspensions
    • G01N15/042—Investigating sedimentation of particle suspensions by centrifuging and investigating centrifugates
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/12—Generating the spectrum; Monochromators
    • G01J3/18—Generating the spectrum; Monochromators using diffraction elements, e.g. grating
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01J—MEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J3/00—Spectrometry; Spectrophotometry; Monochromators; Measuring colours
    • G01J3/12—Generating the spectrum; Monochromators
    • G01J3/18—Generating the spectrum; Monochromators using diffraction elements, e.g. grating
    • G01J2003/1842—Types of grating
    • G01J2003/1857—Toroid surface
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N15/04—Investigating sedimentation of particle suspensions
    • G01N15/042—Investigating sedimentation of particle suspensions by centrifuging and investigating centrifugates
    • G01N2015/045—Investigating sedimentation of particle suspensions by centrifuging and investigating centrifugates by optical analysis

Definitions

  • This invention relates to centrifuges.
  • this invention relates to an optical scanning system for dynamically tracking the progress of stratification within a sample while the centrifuging process occurs.
  • a centrifuge rotor with a sample cell and to observe the sample cell while centrifuging occurs.
  • a light source has been collimated.
  • the collimated light impinges downwardly through the sample cell through upper and lower windows.
  • the collimated light passes precisely parallel to planes of sample stratification at the sample point.
  • the imaging system refocuses the sample image into the plane of a scanning slit.
  • the light passes through an interference filter as it passes to the scanning slit.
  • a photodetector immediate the scanning slit enables detection of bands dynamically while centrifuging is underway.
  • a centrifuge sample is optically scanned during centrifuging.
  • the sample placed in a centrifuge rotor having a cell with windows preferably top and bottom windows, is spun until stratification and discrete layering occurs within the sample.
  • stratification and discrete layering occurs within the sample.
  • Such layers or strata are precisely normal to the radius of the centrifuge at the point of sample and parallel to the spin axis of the centrifuge.
  • Light source is collimated in one plane only. This plane is the sample plane and includes the spin axis of the centrifuge and passes through the sample.
  • the collimated rays pass precisely parallel to the spin axis of the centrifuge across and through layers or strata in the sample.
  • the light is both collimated and chromatically filtered by a toroidal mirror having two curvatures.
  • the cylindrical shape of the mirror with respect to one radius of curvature effects collimation.
  • the rulings of the mirror with respect to the other radius of curvature effect chromatic classification.
  • the light is chromatically filtered and not collimated in the plane perpendicular to the sample plane.
  • a slit scanner having a slit normal to the sample plane traverses the width of the sample below the cell. This traversing slit scanner detects with precision the precise location of the strata in the cell.
  • a preferred optical path including a point source of strobed light of high intensity in the range of 20,000 watts.
  • the point source of light is projected through an aperture 1 mm or less in diameter. This light becomes incident upon a toroidally concave diffraction grating overlying the point of cell sample.
  • the grating is pivoted with cylindrical sections in the sample plane. The grating acting also as a mirror effects collimation in the sample plane precisely normal to the forming strata in the rotating sample.
  • Cylindrical section curvature is such that collimation is not effected when the grating is rotated about its axis of rotation.
  • the mirror is ruled as a diffraction grating along lines perpendicular to the sample plane.
  • the sample is strobed by the light at the time of passage of the cell at the sample point.
  • Light from the light source is incident upon the mirror overlying the cell and is chromatically classified.
  • the light passes through the cell in a band of about 5 nanometers to a lower slit scanning detector with an underlying photodetector.
  • the slit scanning detector in combination with the photodetector precisely locates strata forming within the cell during centrifuging.
  • the mirror can be tilted on an axis included in the plane including the spin axis and radius at the point of sample.
  • This axis of mirror tilt is preferably at right angles to the spin axis of the rotor.
  • the mirror is given unequal spaced rulings so that simple tilt provides the desired chromatic output without the necessity of adjusting the focal length of the mirror with respect to the sample to obtain the chromatically classified light.
  • An object of this invention is to increase the illumination intensity of a sample undergoing process by spinning in a centrifuge.
  • an apertured light source is strobed at the instant a sample is to be taken.
  • Light from the light source is incident upon a mirror immediately overlying the sample.
  • the mirror is provided with a preferably cylindrical surface in a plane including the spin axis of the centrifuge and the radius of the sample point.
  • Light is reflected downwardly from the mirror collimated precisely parallel to the spin axis of the centrifuge and in a sample plane including the sample point and the spin axis of the rotor.
  • a slit scanning detector disposed normally to the sample plane has excursion back and forth under the sample. This detector precisely identifies layers of stratification by their optical absorption as they are dynamically formed in the centrifuging process.
  • An advantage of collimating the scanning light only in the sample plane including the spin axis of the rotor and the sample point is that illumination from the light source is more efficiently used. For example, it is possible to illuminate the sample with ten times that illumination which-would be available if the sample was illuminated by a normally collimated beam, the normally collimated beam including collimation transverse of the sample plane.
  • a further advantage of the scanning system herein disclosed is that extremely narrow bands may be dynamically tracked while they are classified out of the sample.
  • the sedimentation process of the bands (for example their sedimentation coefficient) can be actively followed.
  • a further advantage of the disclosed collimation is that it eliminates the need for an imaging system to refocus the cell to the plane of the image detector. This allows operation with resolution in steep sample refraction gradients.
  • a further object of this invention is to disclose an apparatus which enables the sample to be chromatically scanned at different wavelengths during the centrifuging process.
  • the mirror is ruled and curved.
  • the mirror is provided with conventional unequally spaced rulings. These rulings are supplied to obviate the necessity of changing the mirror to sample distance for differing sampling wavelenghts.
  • An advantage of this aspect of the invention is that by simply tilting the mirror on which the light source is incident varies the wavelength of the light scanning the sample.
  • a further advantage of this ruled mirror is that it preserves the efficient use of light at the sample by avoiding collimation of the light in the plane of the strata formed in the sample. Increased illumination is maintained at the sample.
  • a further object of this invention is to disclose a folded optical path having a long light path from the source to the sample and a short light path from the sample to the detector.
  • An advantage of this aspect of the invention is that the sample is examined with large depth of field by almost perfectly parallel light rays regardless of the angular position of the grating. At the same time the sample, once examined, is immediate the detector. Little degradation of the optical image of the sample to the slit detector occurs.
  • a so-called "ultracentrifuge” is illustrated.
  • a motor M spins a rotor R about an axis A. High speeds are involved. It is not uncommon for rotor R to spin at 100,000 revolutions/minute. As is well known in the art, centrifuging occurs in a vacuum to avoid windage.
  • a sample is contained within a cell S1.
  • the cell includes an upper window 20 and a lower window 22 permitting light to pass parallel to the spin axis of rotor R. It is through these respective windows that a light sample formed in accordance with the teaching of this invention performs the method of examining sample stratification while centrifuging dynamically occurs.
  • detector D is a moving slit capable of having excursion over the radial length of the sample.
  • sample is typically disposed at a sample point P when the sample is optically read for stratification.
  • Sample point P lies along a radius 26 from the spin axis A of the centrifuge.
  • a sample plane includes the spin axis A and the radius 26 extending from the spin axis through the point of sample. This sample plane is the plane in which the light collimation occurs. This same sample plane is the plane of Fig. 4.
  • This plane is the dispersion plane and is the plane along which chromatic dispersion of light occurs. Collimation of light does not occur in the dispersion plane.
  • This dispersion plane is the plane of the illustration of Fig. 3.
  • the function of the specialized optics of this invention can be set forth. This function will include first the collimation of the light to produce the desired examination of the strata along the sample plane. Secondly, the chromatic classification of the light will be discussed with respect to the dispersion plane. Finally, and with reference to Fig. 5. the resolution characteristics of the invention will be set forth.
  • a strobed light source L passes an aperture 28 preferably 1 mm or less in diameter.
  • Light 40 from the light source passes respective tube stops 30 and 32 and is incident upon mirror M.
  • Fig. 4 the reader will understand that light source L is not shown, Fig. 4, however, does show light 40 emanating downwardly from mirror M through sample 50 past a slit detector 52 and to and upon a detector D. It will be understood that slit 52 scans underneath the sample 50. In such scanning it will identify strata precisely parallel to spin axis A and normal to the sample plane of Fig. 4.
  • Mirror M is here shown given a cylindrical shape with respect to light source L in the sample plane of Fig. 4. This cylindrical shape is chosen so that rays 40 are precisely collimated within the plane of Fig. 4 along a path parallel to the spin axis of rotor R. Thus, any classified layers of sediment such as that existing at band B have the collimated rays 40 past precisely parallel to and through the band B.
  • Mirror M is shaped along one axis for the generation of the collimated rays. Along the other axis, the mirror is provided with a different curvature and differently spaced rulings so that tilting of the mirror produces light of varying color.
  • Rotation of grating to change wavelength occurs about 30° from normal to the light source. Effective curvature for collimation does not charge regardless of grating angle.
  • slit 52 traverses the detector D back and forth along the path indicated by double arrow 54.
  • detector D will see the differences in the receipt of light as described in Cohen U.S. Patent 3,712,742 issued January 23, 1973.
  • light source L is typically a strobed zenon source. At the instant of strobing the light source includes output in the range of 20,000 watts.
  • mirror M is provided with curvatures having unequal spaced rulings in the plane of Fig. 4. As viewed in Fig. 3, the rulings extend into and out of the plane of the drawing.
  • scanning of sample 50 can occur in 5 nanometer wide bands.
  • the width of the scanning optical bands or band pass is in effect determined by the solid angle of mirror radiation defined through windows 20, 22 as viewed in Figs. 3 and 4.
  • Serendipity is present from such scanning.
  • the band of chromatically classified light is parallel to and in the plane of the band B as shown in Fig. 4.
  • both the-band B and its respective surfaces are illuminated with light.
  • the illuminating light is in the order of ten times that light which would be available had the light been collimated with respect to both the planes of Figs. 3 and 4.
  • FIG. 5 an optical schematic of the system is illustrated. This schematic demonstrates how the length of the folded light path illustrated in Figs. 3 and 4 assists in the band resolution of the sample.
  • the distance X1 represents the effective length of the optical path between the light L and the sample S1. This distance is equal to about 33 cm.
  • the distance X2 is the distance between the slit 52 and the sample S1. This distance is about 2 cm. It will be observed that the folded light path X1 is very much longer than the path X2. Therefore. the slit 52 will see the banding B at a high resolution where: d2 X2 ⁇ d1 X1
  • FIG. 6 the optical tube in the vicinity of the mirror schematically shown in Figs. 3 and 4 is illustrated.
  • the mirror is shown in the same plane as the schematic of Fig. 4.
  • Optical baffles eliminate all portions of the beam from light L (See Fig. 1) save and except that light which will impact mirror M. Light is reflected from mirror M and passes down tube T1 to sample the contents of a rotating cell.
  • Mirror M pivots about a pivot 102.
  • the mirror is driven in such pivotal motion by a gear train including gears 103, 104.
  • This gear train also includes reduction gears 105, 106, an idler gear 107 which is finally driven by a rack 108.
  • rack 108 As can be readily understood, by linear motion of rack 108 towards and away from the mirror, finely adjusted and precise rotation of mirror M can occur. Since the mirror always collimates, change in angle of the mirror will only affect the color doing the sampling at the rotating cell.
  • the ability to rapidly change color enables the rapid adjustment of the color for sampling the classified materials within the cell.
  • the photodetector passes over the radius of an individual cell, the color of the sampling light can be rapidly changed for optimum detection of classified strata having varying optical densities.
  • slit 52 and the detector D as shown in Fig. 4 has an additional advantage that is not apparent. Specifically, as sample S1 is increasing classified, various components of the sample will settle out at discrete layers. These components can include various salts.
  • slit 52 has an active width of approximately 0.1 millimeter and is spaced with respect to the active surface of detector D so that a plus or minus 2 degree from the vertical angular view of the sample is obtained.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • General Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Centrifugal Separators (AREA)
  • Optical Measuring Cells (AREA)
EP88909862A 1987-10-29 1988-10-20 Uv scanning system for centrifuge Expired EP0340279B1 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US07/115,023 US4830493A (en) 1987-10-29 1987-10-29 UV scanning system for centrifuge
US115023 1987-10-29

Publications (2)

Publication Number Publication Date
EP0340279A1 EP0340279A1 (en) 1989-11-08
EP0340279B1 true EP0340279B1 (en) 1992-08-26

Family

ID=22358870

Family Applications (1)

Application Number Title Priority Date Filing Date
EP88909862A Expired EP0340279B1 (en) 1987-10-29 1988-10-20 Uv scanning system for centrifuge

Country Status (8)

Country Link
US (1) US4830493A (2)
EP (1) EP0340279B1 (2)
JP (1) JPH0742121Y2 (2)
CN (1) CN1011554B (2)
CA (1) CA1295031C (2)
DE (1) DE3874125T2 (2)
HU (1) HU206771B (2)
WO (1) WO1989003986A1 (2)

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GB9302673D0 (en) * 1993-02-11 1993-03-24 Haematest Limited Apparatus for analysing blood and other samples
US5563333A (en) * 1995-01-20 1996-10-08 Haines; Hiemi K. Method and apparatus for core flooding studies
US7173551B2 (en) 2000-12-21 2007-02-06 Quellan, Inc. Increasing data throughput in optical fiber transmission systems
US7307569B2 (en) * 2001-03-29 2007-12-11 Quellan, Inc. Increasing data throughput in optical fiber transmission systems
US7149256B2 (en) * 2001-03-29 2006-12-12 Quellan, Inc. Multilevel pulse position modulation for efficient fiber optic communication
IL158211A0 (en) * 2001-04-04 2004-05-12 Quellan Inc Method and system for decoding multilevel signals
US20030030873A1 (en) * 2001-05-09 2003-02-13 Quellan, Inc. High-speed adjustable multilevel light modulation
WO2003071731A1 (en) * 2002-02-15 2003-08-28 Quellan, Inc. Multi-level signal clock recovery technique
US6816101B2 (en) * 2002-03-08 2004-11-09 Quelian, Inc. High-speed analog-to-digital converter using a unique gray code
AU2003223687A1 (en) * 2002-04-23 2003-11-10 Quellan, Inc. Combined ask/dpsk modulation system
JP2004013681A (ja) * 2002-06-10 2004-01-15 Bosu & K Consulting Kk 名刺情報管理システム
US7035361B2 (en) * 2002-07-15 2006-04-25 Quellan, Inc. Adaptive noise filtering and equalization for optimal high speed multilevel signal decoding
AU2003287628A1 (en) * 2002-11-12 2004-06-03 Quellan, Inc. High-speed analog-to-digital conversion with improved robustness to timing uncertainty
JP2007502054A (ja) * 2003-08-07 2007-02-01 ケラン インコーポレイテッド クロストークキャンセルのための方法とシステム
US7804760B2 (en) * 2003-08-07 2010-09-28 Quellan, Inc. Method and system for signal emulation
ATE488068T1 (de) * 2003-11-17 2010-11-15 Quellan Inc Verfahren und system zur löschung von antennenstörungen
US7616700B2 (en) * 2003-12-22 2009-11-10 Quellan, Inc. Method and system for slicing a communication signal
US7209230B2 (en) 2004-06-18 2007-04-24 Luckoff Display Corporation Hand-held spectra-reflectometer
US7725079B2 (en) * 2004-12-14 2010-05-25 Quellan, Inc. Method and system for automatic control in an interference cancellation device
US7522883B2 (en) * 2004-12-14 2009-04-21 Quellan, Inc. Method and system for reducing signal interference
US20100239436A1 (en) * 2005-05-17 2010-09-23 Honeywell International Inc. A thermal pump
US7233394B2 (en) 2005-06-20 2007-06-19 Luckoff Display Corporation Compact spectrometer
WO2007127369A2 (en) * 2006-04-26 2007-11-08 Quellan, Inc. Method and system for reducing radiated emissions from a communications channel
US20230330686A1 (en) * 2022-04-18 2023-10-19 Fenwal, Inc. Interface Detection And Control Using A Photodetector Array

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Also Published As

Publication number Publication date
EP0340279A1 (en) 1989-11-08
HU206771B (en) 1992-12-28
CN1039123A (zh) 1990-01-24
CA1295031C (en) 1992-01-28
DE3874125T2 (de) 1993-04-08
CN1011554B (zh) 1991-02-06
HU886712D0 (en) 1990-09-28
DE3874125D1 (de) 1992-10-01
US4830493A (en) 1989-05-16
HUT53736A (en) 1990-11-28
JPH02500028U (2) 1990-07-05
WO1989003986A1 (en) 1989-05-05
JPH0742121Y2 (ja) 1995-09-27

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